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Method for preparing isophorone diamine

A technology of isophorone diamine and isophorone nitrile is applied in the field of preparation and optimization of catalytic reaction process, which can solve the problems of low yield of IPDA, and achieve the effects of long catalyst life, uniform dispersion and high activity

Inactive Publication Date: 2013-08-28
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Gained IPDA yield is lower than 85%, also has more than 15% nitrile amine and secondary amine by-product

Method used

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  • Method for preparing isophorone diamine
  • Method for preparing isophorone diamine
  • Method for preparing isophorone diamine

Examples

Experimental program
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Effect test

Embodiment 1

[0035] Embodiment 1: Sol-gel method prepares metallic cobalt catalyst

[0036] (1) Metal cobalt catalyst with metal cobalt loading of 10wt%:

[0037] According to the ratio of ethyl orthosilicate: absolute ethanol: deionized water = 1:4:10 (the ratio of the amount of substances), measure 37.3ml (0.1665mol) ethyl orthosilicate and add it to 38.9ml of absolute ethanol Alcoholic solution of ethyl orthosilicate made in the medium, weigh 5.48g Co(NO 3 ) 2 ·6H 2 O (0.0188mol) was dissolved in 30.0ml deionized water to make an aqueous solution of cobalt nitrate, and the aqueous solution of cobalt nitrate was slowly added dropwise to the absolute ethanol solution of tetraethyl orthosilicate to make a mixed solution, which was stirred while dropping, 5 The dropwise addition is completed within 1 minute, and after the dropwise addition is completed, use 2mol / L dilute nitric acid and 2mol / L ammonia water to adjust the pH of the mixture to 3.5. After adjusting the pH, put the mixed so...

Embodiment 2

[0041] The preparation process of the catalyst is the same as in Example 1, except that dilute nitric acid and ammonia water are used to adjust the pH to 4 at the end, and other conditions are the same. Add 500mg of the activated cobalt metal catalyst (metal cobalt load: 10wt%) prepared in step (1) into a 100ml autoclave, then add 25ml of anhydrous methanol, 2.5g of isophorone nitrile, and close the reactor The air in the reaction kettle is purged and replaced by nitrogen gas afterward, and then the ammonia gas is passed to make the reaction kettle pressure reach 0.1MPa, and then the hydrogen gas is passed to make the reaction kettle pressure be 8MPa, the reaction temperature is 120° C., and the reaction is 8h. Other operations are the same as in Example 1. The conversion rate of IPN is 100%, and the yield of IPDA is 85.5%.

Embodiment 3

[0043] The preparation process of the catalyst is the same as in Example 1, except that dilute nitric acid and ammonia water are used to adjust the pH=4.5 at the end, and other conditions are the same. Add 750mg of the activated metal cobalt catalyst prepared in step (1) (the metal cobalt load is 10wt%) into a 100ml autoclave, then add 40ml of anhydrous methanol, 2.5g of isophorone nitrile, and close the reactor The air in the reaction kettle is purged and replaced by nitrogen gas afterward, and then the ammonia gas is passed to make the reaction kettle pressure reach 0.1MPa, and then the hydrogen gas is passed to make the reaction kettle pressure be 8MPa, the reaction temperature is 120° C., and the reaction is 8h. Other operations are the same as in Example 1. The conversion rate of IPN is 100%, and the yield of IPDA is 92.2%.

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Abstract

The invention discloses a method for preparing isophorone diamine, wherein the method comprises: using phorone nitrile as a raw material, under an effect of a metal cobalt catalyst, ammonia gas and hydrogen are orderly introduced into an organic solvent, and are reacts under stirring for 1-8h at 40-180 DEG C in a pressure condition of 1-10 MPa, and after reaction, a reaction mixture is post-treated to obtain the isophorone diamine. Uniformly-dispersive and high active metal cobalt catalyst is prepared by a sol-gel method, and when the catalyst is used for preparing isophorone diamine, a conversion rate of IPN can reach 100%, and the yield of IPAD is 78.5-98.3%. The catalyst has a long service life, and after the catalyst repeats eight-time by simple filtration after catalytic reaction, the conversion rate of IPN reduces 6.3%, yield of IPDA reduces 7.8%, and catalyst activity is almost not changed.

Description

(1) Technical field [0001] The present invention relates to a method for preparing isophorone diamine (IPDA for short, CAS: 2855-13-2) by catalytic hydrogenation of isophorone nitrile (IPN for short, CAS: 7027-11-4). The core is the preparation of highly active hydrogenation catalyst and the optimization of catalytic reaction process. (2) Background technology [0002] IPDA is an alicyclic diamine with low color, low viscosity, high strength, and good chemical resistance. It is widely used as a curing agent for epoxy resins, and a chain extender and accelerator for polyurethanes. In recent years, my country's polyurethane industry has entered a period of development, and the development of phenylisocyanate used as raw materials has also continued to grow. Isophorone diisocyanate (IPDI for short, CAS: 4098-71-9) can be obtained by phosgenation of IPDA. Due to its structural characteristics, IPDI has excellent mechanical properties and aging resistance, and is currently grad...

Claims

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Application Information

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IPC IPC(8): C07C211/36C07C209/48C07C209/52B01J23/75
Inventor 魏作君汪梨超刘迎新
Owner ZHEJIANG UNIV
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